CN107936943A - A kind of quantum dot fluorescence intensity enhancing method based on dendrimer - Google Patents
A kind of quantum dot fluorescence intensity enhancing method based on dendrimer Download PDFInfo
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- CN107936943A CN107936943A CN201711264498.2A CN201711264498A CN107936943A CN 107936943 A CN107936943 A CN 107936943A CN 201711264498 A CN201711264498 A CN 201711264498A CN 107936943 A CN107936943 A CN 107936943A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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Abstract
The invention discloses a kind of quantum dot fluorescence intensity enhancing method based on dendrimer.Using dendrimer as stabilizer, realize the Fluorescence Increasing between the two amounts point of different emission, belong to fluorescence analysis field.This method comprises the following steps：A kind of quantum dot is synthesized by stabilizer of dendrimer；Again the different quantum dot of another launch wavelength is synthesized with other stabilizers；Two amounts son point is mixed with different mol ratio, by adjusting mixing molar ratio, it can be achieved that the effect that different wave length quantum dot fluorescence mutually strengthens, so as to improve the sensitivity of quantum dot fluorescence detection method.
Description
Technical field
The present invention relates to fluorescence analysis field, and in particular to a kind of to realize different emission using dendrimer
The method that the fluorescence intensity of two amounts point mutually strengthens.
Background technology
Quantum dot is also known as semiconductor nanocrystals grain, it has the characteristics that wide excitation spectrum, launch wavelength are controllable.Pass through tune
Section quantum dot size can change wavelength of fluorescence, or multiple launch wavelengths detect different material at the same time.Meanwhile quantum dot possesses hair
Light efficiency is high, good light stability and many advantages, such as be not easy photobleaching, and the field such as detecting in biomarker, fluorescence analysis has
It is widely applied prospect.
But biological sample concentration is low, fluorescence is weaker, when quantum dot is used for biological detection, in order to improve the spirit of detection
Sensitivity, it is necessary to strengthen its fluorescence intensity；Since quantum dot size is small, surface energy is higher, easily reunites in preparation process, because
How this, improve quantum dot preparation method, reduces quantum dot and reunites and improve its fluorescence intensity and stability, is quantum dot application
With the key issue of popularization.
The content of the invention
To achieve these goals, the present invention provides a kind of quantum dot fluorescence intensity enhancing side based on dendrimer
Method.
The quantum dot fluorescence intensity enhancing method based on dendrimer is achieved through the following technical solutions：
A kind of quantum dot fluorescence intensity enhancing method based on dendrimer, includes the following steps：
(1) using dendrimer the first quantum dot is synthesized for stabilizer；
(2) with the second different quantum dot of other stabilizers synthesis launch wavelength；
(3) by the point mixing of two amounts, realize that different wave length quantum dot fluorescence mutually strengthens by regulating and controlling its molar ratio.
Preferably, the preparation of first quantum dot includes the steps：
(1) it is 1.0 × 10 to concentration-41.0 × 10 are added in mol/L dendrimer solution-3The Zn of mol/L2+、Cd2+、Hg2 +Or Cu2+Deng metal ion solution, Zn2+、Cd2+、Hg2+Or Cu2+Ion and dendrimer molar ratio are (1-20):1, the pH of solution
For 6.8-7.2, after being ultrasonically treated 1-3h, being stirred at room temperature makes Zn2+、Cd2+、Hg2+Or Cu2+Ion is balanced with dendrimer coordination, is obtained
To metal ion and the complex solution of dendrimer；
(2) S equal with metal ion is added into the solution of step (1)2-、Se2-Or Te2-Solion,
The quantum dot solution for reacting 1-3h at 0-10 DEG C and dendrimer parcel being made, dialysis purification, Cord blood.
Preferably, the kernel of the dendrimer in the step (1) is ethylenediamine, acrylonitrile, 2-aminoethyl disulfide dihydrochloride or three
Monoethanolamine.
Preferably, the dendrimer in the step (1) is 4 global molecular more than generation, has ammonia in its crotch structure
Base；The end group of the dendrimer is amino, carboxyl, hydroxyl or ester group.
Preferably, the metal ion solution in the step (1) and step (2) is molten using the mixing of methanol, water or both
Liquid.
Preferably, the preparation of second quantum dot includes the steps：
(1)Zn2+、Cd2+Or Hg2+As cation precursor solution, Se2-、Te2-Or S2-It is molten as anion presoma
Liquid；
(2) thioacetic acid, mercaptopropionic acid, mercaptoethanol, mercaptoethylmaine, glutathione, cysteine, thiocarbamide or sulphur are added
The common stabilizer such as Pu Luoning, adjusts pH, is heated to reflux precursor mixed solution and prepares quantum dot.
Preferably, the step (3) specifically includes the steps：
The first quantum dot and the second quantum dot of certain volume are taken, makes the molar ratio of two amounts point at (0.1-50):1,
Deionized water is settled to same volume.
The present invention is a kind of quantum dot fluorescence intensity enhancing method based on dendrimer, is mainly exaggerated the glimmering of quantum dot
Optical signal, has the characteristics that；Quantum dot is synthesized using the internal cavity of dendrimer, a dendrimer can accommodate multiple amounts
It is sub-, it is exaggerated the fluorescence signal of single quantum dot；Utilize the branch structure of dendrimer, it is possible to reduce quantum dot self collision energy
Amount loss, strengthens the fluorescence intensity of quantum dot；The quantum dot synthesized using dendrimer used as stabilizers, size uniform, dispersiveness
It is good, by adjusting the molar ratio of metal ion and dendrimer, the size of quantum dot can be effectively controlled, realizes quantum dot emission
Wavelength it is adjustable controllable；The quantum dot synthesized using dendrimer, surface carry substantial amounts of functional group, being capable of external a variety of things
Matter, and dendrimer bio-compatibility is good, and the quantum dot that can be synthesized is applied to biological field；Closed using dendrimer
Into a kind of quantum dot, synthesized with other stabilizers another quantum dot mixing, by control mixing molar ratio, reach not
The effect that co-wavelength quantum dot fluorescence mutually strengthens；The two amounts point of the present invention can design probe in pairs, for examining at the same time
Survey two kinds of materials.
Brief description of the drawings
Fig. 1 is schematic diagram provided by the invention.
Fig. 2 is the CdTe/CdS quantum dots for the various concentrations that the present invention provides embodiment one to CdS-PAMAM quantum dots
Fluorescence Increasing design sketch.
Fig. 3 is the CdS-PAMAM quantum dots for the various concentrations that the present invention provides embodiment one to CdTe/CdS quantum dots
Fluorescence Increasing design sketch.
Fig. 4 be the present invention provide embodiment one CdS-PAMAM quantum dots and CdTe/CdS quantum dots using molar ratio as
4.7:The design sketch of 1 mixing.
Fig. 5 is the CdSe/ZnS quantum dots for the various concentrations that the present invention provides embodiment two to CdS-PAMAM quantum dots
Fluorescence Increasing design sketch.
Fig. 6 is the CdS-PAMAM quantum dots for the various concentrations that the present invention provides embodiment two to CdSe/ZnS quantum dots
Fluorescence Increasing design sketch.
Fig. 7 be the present invention provide embodiment two CdS-PAMAM quantum dots and CdSe/ZnS quantum dots using molar ratio as
3.7:The design sketch of 1 mixing.
Embodiment
Technical scheme is described in detail below by specific embodiment, but the scope of the present invention is not
It is limited to these embodiments.
Specific embodiment 1
A kind of quantum dot fluorescence intensity enhancing method based on dendrimer is present embodiments provided, specifically includes following step
Suddenly：
(1) the pamam dendrimer molecule using 4.0 ends of G as amino is inner template synthesis CdS quantum dot：It is 1.0 toward concentration
×10-41.0 × 10 are added in mol/L pamam dendrimer molecule methanol solutions-3Mol/L caddy methanol solutions, (n Cd2+:n
PAMAM=10:1) pH for, adjusting solution is about 7.0, and then ultrasound 1h, is then stirred at room temperature 24h, obtains Cd2+Ion with
The complex solution of pamam dendrimer molecule；Again toward adding S in complex solution2-Ion methanol solution, (n Cd2+:nS2-=1:1), so
1h being reacted at 4 DEG C afterwards and obtaining the CdS quantum dot solution of dendrimer parcel, quantum dot is finally subjected to dialysis purification, is put in ice
4 DEG C of preservations of case；
(2) CdTe/CdS core-shell quanta dots are synthesized：
Synthesize NaHTe presomas：By 0.0638gTe powder and 0.0420g NaBH41mL deionized waters are dissolved in, stirring is anti-
Should be colourless transparent solution to upper strata, lower floor is white powder.
Synthesize CdTe cores：By 0.0285gCdCl2·2.5H2O is dissolved in 25mL deionized waters；Add 20.5 μ L thioacetic acid
(MPA), pH is adjusted to 9.0-11.0,15 μ LNaHTe presomas is added under the protection of nitrogen, then lead to N215min, is put into
4 DEG C of refrigerator is kept in dark place, overnight.
Synthesize shell：2.4mL, 25mmol/L Cd are added into three-necked flask2+/ MPA mixed liquors, (n Cd2+:NMPA=1:
2), and 17.6mLCdTe cores, pH is adjusted to 9.0-11.0,8h is reacted at 90 DEG C, 4 DEG C of refrigerator is then put and is kept in dark place.
(3) the Fluorescence Increasing optimum mole ratio of CdS-PAMAM quantum dots is probed into
100 μ LCdS-PAMAM quantum dots are added into 1.5mL centrifuge tubes, (parallel to add 4 parts), adds different volumes
CdTe/CdS core-shell quanta dots, are finally settled to 200 μ L with deionized water, make CdTe/CdS quantum dots and CdS-PAMAM amounts
The molar ratio of son point mixing is respectively 0.06:1、0.1:1、0.17:1、0.2:1, the fluorescence of mixed solution is then measured, with
The increase of the amount of CdTe/CdS core-shell quanta dots, the fluorescence of CdS-PAMAM gradually strengthen, when molar ratio is 0.2:Reach pole when 1
Value, it is 0.2 that continuing, which increases the amount of CdTe/CdS core-shell quanta dots and molar ratio,:When 1 consistent (the results are shown in Figure 2)；
(4) the Fluorescence Increasing optimum mole ratio of CdTe/CdS quantum dots is probed into
100 μ LCdTe/CdS core-shell quanta dots are added into 1.5mL centrifuge tubes, (parallel to add 4 parts), adds different volumes
CdS-PAMAM quantum dots, be finally settled to 200 μ L with deionized water, make CdS-PAMAM quantum dots and CdTe/CdS nucleocapsids
Quantum dot mixing molar ratio be respectively：0.5:1、1:1、3:1、4:1, the fluorescence of mixed solution is then measured, with CdS-
The increase of the amount of PAMAM quantum dots, the fluorescence of CdTe/CdS gradually strengthen, when molar ratio is 4:Reach extreme value when 1, continue to increase
The amount of CdS-PAMAM quantum dots is 4 with molar ratio:When 1 consistent (the results are shown in Figure 3)；
(5) Fig. 4 is CdS-PAMAM quantum dots and CdTe/CdS quantum dots using molar ratio as 4.7:The fluorescent effect of 1 mixing
Figure, and it is diluted to the CdS-PAMAM quantum dots and CdTe/CdS quantum dot blank fluorescence figures of same concentrations.
Specific embodiment 2
Present embodiments provide a kind of a kind of enhancing quantum dot fluorescence intensity method based on dendrimer, specifically include as
Lower step：
(1) the pamam dendrimer molecule using G4.0 ends as amino is inner template synthesis CdS quantum dot (with reference to embodiment 1)；
(2) CdSe/ZnS quantum dot (bibliography is synthesized[1])：
Synthesize NaHSe presomas：By 0.0316g Se powder and 0.0632g NaBH4It is dissolved in 1mL deionized waters, stirs
Reaction to black powder disappears.
Synthesize CdSe/ZnS quantum dots：40mL, 0.02mol/L cadmium chlorates and 0.21mL MPA are added toward three-necked flask, is adjusted
It is (9.0-11.0) to save pH value of solution, adds 1mL NaHSe presomas under nitrogen protection, and the solution is heated 3h in 96 DEG C.So
Afterwards, the 0.01mol/L vulcanized sodium of the 0.01mol/L zinc acetates of 2mL and 2mL is alternately added in above-mentioned solution.Final is molten
Liquid continues the 48h that flows back at 96 DEG C, then puts 4 DEG C of refrigerator and is kept in dark place.
(3) the Fluorescence Increasing optimum mole ratio of CdS-PAMAM quantum dots is probed into
100 μ L CdS-PAMAM quantum dots are added into 1.5mL centrifuge tubes, (parallel to add 4 parts), adds different volumes
CdSe/ZnS quantum dots, are finally settled to 200 μ L with deionized water, make CdSe/ZnS quantum dots and CdS-PAMAM quantum dots
The molar ratio of mixing is respectively：1:0.13、1:0.19、1:0.25、1:0.38, the fluorescence of mixed solution is then measured, with
The increase of the amount of CdSe/ZnS core-shell quanta dots, the fluorescence of CdS-PAMAM gradually strengthen, when molar ratio is 1:Reach pole when 0.38
Value, it is 1 that continuing, which increases the amount of CdSe/ZnS core-shell quanta dots and molar ratio,:When 0.38 consistent (the results are shown in Figure 5)；
(4) the Fluorescence Increasing optimum mole ratio of CdSe/ZnS quantum dots is probed into
100 μ LCdSe/ZnS quantum dots are added into 1.5mL centrifuge tubes, (parallel to add 4 parts), adds different volumes
CdS-PAMAM quantum dots, are finally settled to 200 μ L with deionized water, make CdS-PAMAM quantum dots and CdSe/ZnS quantum dots
The molar ratio of mixing is respectively：0.53:1、1.1:1、1.6:1、3.7:1, the fluorescence of mixed solution is then measured, with CdS-
The increase of the amount of PAMAM quantum dots, the fluorescence of CdSe/ZnS gradually strengthen, when molar ratio is 3.7:Reach extreme value when 1, continue to increase
It is 3.7 to add the amount of CdSe/ZnS quantum dots and molar ratio:When 1 consistent (the results are shown in Figure 6)；
(5) Fig. 7 is CdS-PAMAM quantum dots and CdSe/ZnS quantum dots using molar ratio as 3.7:The fluorescent effect of 1 mixing
Figure, and it is diluted to the CdS-PAMAM quantum dots and CdSe/ZnS quantum dot blank fluorescence figures of same concentrations.
Embodiment above is only the preferred embodiments of the invention, it should be pointed out that, come for ordinary skill people
Say, what is carried out under the premise of not departing from the present invention is partially improved, among protection scope of the present invention.
Claims (7)
1. a kind of quantum dot fluorescence intensity enhancing method based on dendrimer, it is characterised in that including the steps：
(1) using dendrimer the first quantum dot is synthesized for stabilizer；
(2) with the second different quantum dot of other stabilizers synthesis launch wavelength；
(3) two amounts point is mixed with different mol ratio, by regulating and controlling molar ratio, realizes different wave length quantum dot fluorescence intensity
Mutual enhancing effect.
2. the quantum dot fluorescence intensity enhancing method according to claim 1 based on dendrimer, it is characterised in that：It is described
Step (1) specifically includes the steps：
Zn is added into dendrimer solution2+、Cd2+、Hg2+Or Cu2+Deng metal ion, Zn2+、Cd2+、Hg2+Or Cu2+Ion and tree
Shape molecule molar ratio is (1-20):1；Adjust solution pH be 7 or so, be ultrasonically treated 1-3h after, obtain metal ion with it is tree-like
The complex solution of molecule.The S equal with metal ion is added into above-mentioned complex solution2-、Se2-Or Te2-Ion is molten
Liquid, reacts 1-3h at 0-10 DEG C, the quantum dot solution of dendrimer parcel, dialysis purification, Cord blood is made.
3. the quantum dot fluorescence intensity enhancing method according to claim 2 based on dendrimer, it is characterised in that：It is described
The kernel of dendrimer is ethylenediamine, acrylonitrile, 2-aminoethyl disulfide dihydrochloride or triethanolamine.
4. the quantum dot fluorescence intensity enhancing method according to claim 3 based on dendrimer, it is characterised in that：It is described
Dendrimer is 4 global molecular more than generation, has amino in its crotch structure；The end group of the dendrimer is ammonia
Base, carboxyl, hydroxyl or ester group.
5. the quantum dot fluorescence intensity enhancing method according to claim 4 based on dendrimer, it is characterised in that：It is described
Metal ion solution uses the mixed solution of methanol, water or both.
6. according to any quantum dot fluorescence intensity enhancing methods based on dendrimer of claim 1-5, its feature exists
In：The synthesis step of second quantum dot is as follows：
(1)Zn2+、Cd2+Or Hg2+As cation precursor solution, Se2-、Te2-Or S2-As anion precursor solution；
(2) thioacetic acid, mercaptopropionic acid, mercaptoethanol, mercaptoethylmaine, glutathione, cysteine, thiocarbamide or general sieve of sulphur are added
The common stabilizer such as peaceful, adjusts pH, is heated to reflux precursor mixed solution and prepares quantum dot.
7. the quantum dot fluorescence intensity enhancing method according to claim 6 based on dendrimer, it is characterised in that：It is described
In step (3), the molar ratio of the first quantum dot and the second quantum dot is (0.1-50):1, with deionized water constant volume.
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Cited By (4)
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| WO2020108077A1 (en) * | 2018-11-28 | 2020-06-04 | Tcl科技集团股份有限公司 | Quantum dot color filter and manufacturing method therefor |
| CN111234802A (en) * | 2018-11-28 | 2020-06-05 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN111234804A (en) * | 2018-11-28 | 2020-06-05 | Tcl集团股份有限公司 | Preparation method of quantum dots |
| CN112961365A (en) * | 2021-02-03 | 2021-06-15 | 宁波大学 | Novel method for enhancing fluorescence property of metal organic framework material |
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Cited By (4)
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| WO2020108077A1 (en) * | 2018-11-28 | 2020-06-04 | Tcl科技集团股份有限公司 | Quantum dot color filter and manufacturing method therefor |
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| CN112961365A (en) * | 2021-02-03 | 2021-06-15 | 宁波大学 | Novel method for enhancing fluorescence property of metal organic framework material |
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Application publication date: 20180420 |